CN101638248A - Method and system for recovering residual titanium tetrachloride in copper-wire tower - Google Patents
Method and system for recovering residual titanium tetrachloride in copper-wire tower Download PDFInfo
- Publication number
- CN101638248A CN101638248A CN200810012580A CN200810012580A CN101638248A CN 101638248 A CN101638248 A CN 101638248A CN 200810012580 A CN200810012580 A CN 200810012580A CN 200810012580 A CN200810012580 A CN 200810012580A CN 101638248 A CN101638248 A CN 101638248A
- Authority
- CN
- China
- Prior art keywords
- titanium tetrachloride
- vacuum
- copper
- valve
- wire tower
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 68
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000011084 recovery Methods 0.000 claims abstract description 14
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 12
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000029058 respiratory gaseous exchange Effects 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 5
- 230000003139 buffering effect Effects 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 230000008929 regeneration Effects 0.000 claims description 6
- 238000011069 regeneration method Methods 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 230000000241 respiratory effect Effects 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 3
- NXMBUZSTCIMOMW-UHFFFAOYSA-J [Cu].[Ti](Cl)(Cl)(Cl)Cl Chemical compound [Cu].[Ti](Cl)(Cl)(Cl)Cl NXMBUZSTCIMOMW-UHFFFAOYSA-J 0.000 abstract description 2
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 4
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- QLOKAVKWGPPUCM-UHFFFAOYSA-N oxovanadium;dihydrochloride Chemical compound Cl.Cl.[V]=O QLOKAVKWGPPUCM-UHFFFAOYSA-N 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for removing vanadium from a titanium tetrachloride copper wire, and in particular relates to a method and a system for recovering residual titanium tetrachloride in acopper-wire tower. In the method for recovering the residual titanium tetrachloride in the copper-wire tower, a breathing pipeline on the rear of a secondary condenser in the prior copper-wire towervanadium removal process is provided with a branch and is connected with a vacuum system, the residual titanium tetrachloride in the copper-wire tower is recovered before copper-wire ball regenerationtreatment, the negative pressure generated by the vacuum system makes the residual titanium tetrachloride in the copper-wire tower evaporated into a condenser by means of self vapor pressure, and thetitanium tetrachloride is condensed due to the low temperature of the condenser and the secondary condenser, and is collected to a condensate buffer storage tank. The method can recover the residualtitanium tetrachloride in the copper-wire tower and reduce the loss of the titanium tetrachloride to improve the recovery efficiency of materials, prolongs the service life of the copper-wire tower, and reduces the quantity of waste acid water.
Description
Technical field
The present invention relates to a kind of method of titanium tetrachloride copper wire vanadium removal, especially relate to a kind of method and system thereof that reclaims residual titanium tetrachloride in copper-wire tower.
Background technology
In the copper wire vanadium removal process, the vanadylic chloride (VOCl in the titanium tetrachloride
3) can following reaction take place with copper:
TiCl
4+Cu＝CuCl·TiCl
3
CuCl·TiCl
3+VOCl
3＝VOCl
2↓+CuCl+TiCl
4
After removing vanadium and carrying out for some time, the copper wire surface can be chlorinated cuprous and vanadyl dichloride wraps and lose chemically reactive, at this moment needs copper wire is carried out manipulation of regeneration, makes its surface have chemically reactive again.Current methods is to wash copper wire balls at copper wire tower bubble, and the titanium tetrachloride and the water that remain on the copper wire balls can produce following hydrolysis reaction generation metatitanic acid and hydrochloric acid: TiCl
4+ 3H
2O=H
2TiO
3+ 4HCl.
Because hydrochloric acid (HCl) can produce pitting attack to the copper wire tower of stainless steel, can influence the copper wire tower life-span with this method, also produces a large amount of waste acid waters simultaneously.Some factory directly emits the copper wire balls that has titanium tetrachloride for protection copper wire tower; because titanium tetrachloride and water in air distribution unboiled water are separated reaction and are generated white vaporific hydrochloric acid gas; make that Working environment is very abominable in the workshop, hydrochloric acid is also quite serious to the corrosion of workshop factory building and device outer surface simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of method that reclaims residual titanium tetrachloride in copper-wire tower, be used to prolong the life-span of copper wire tower, reduce waste acid water, improve Working environment in the workshop.
Be achieved in that a kind of method that reclaims residual titanium tetrachloride in copper-wire tower for reaching above-mentioned purpose the present invention, respiratory siphon pass after original copper wire tower is except that secondary condenser in the vanadium technology goes out branch, and connection vacuum system, before the copper wire balls manipulation of regeneration, titanium tetrachloride residual in the copper wire tower is reclaimed, the negative pressure of utilizing vacuum system to produce makes the titanium tetrachloride that remains in the copper wire tower lean on the vapour pressure of self to be evaporated to condenser, because the low temperature of condenser and secondary condenser makes titanium tetrachloride be condensed and is collected into phlegma buffering storage tank.
The method of described recovery residual titanium tetrachloride in copper-wire tower, it is heating power supply and the valve 1 and the flow control valve 2 of closing still kettle 3 earlier, open underflow valve 4 the more a part of titanium tetrachloride in titanium tetrachloride in the still kettle 4 and the copper wire tower 6 is expelled to except that titanium tetrachloride storage tank before the vanadium, close underflow valve 4 then; Shut-off valve 10 and valve 11 are also opened valve 12, start vacuum pump 19, and the vacuum tightness of measuring according to the vacuumometer on the vacuum buffer tank 16 15 and control vacuum breaker 17 is automatically closed sky variable valve 17 automatically after vacuum tightness reaches requirement; Valve 12 places behind secondary condenser are provided with vacuumometer 13, automatically control vacuum breaker 14 according to the vacuum tightness of measuring, making herein that vacuum tightness is neither too high lowly only (is pressed with the pass with titanium tetrachloride vapors under the differing temps, when temperature was in 10～50 ℃, vacuum tightness should be at 700～5000Pa; When temperature was in 50～136 ℃, vacuum tightness should be 5000～50000Pa); Titanium tetrachloride in the copper wire tower is at vacuum and normal temperature or be higher than under the state of normal temperature by self vapour pressure effect and become steam, vapour temperature descends because of the heat-eliminating medium effect after steam enters condenser 7 and 8, because temperature reduction titanium tetrachloride vapors is pressed also reduction to make gaseous titanium tetrachloride be condensed into liquid state and is collected into phlegma buffering storage tank 9, recovery operation is finished.
Thereby the valve 11 of then opening that the vacuum tightness of described measurement is too high makes the argon gas of breathing in the piping system enter reduction vacuum tightness.
After described recovery operation is finished, close vacuum breaker 17, close vacuum pump 19; Open valve 11, open underflow valve 18 then, emit and may enter in the vacuum buffer tank 16 and the titanium tetrachloride that condenses and, shut-off valve 18 again; Close vacuum breaker 14 and valve 12.
The system architecture that reclaims residual titanium tetrachloride in copper-wire tower is as follows: it comprises still kettle 3, copper wire tower 6, first-stage condenser 7, secondary condenser 8 and phlegma buffering storage tank 9, wherein connect breathing pipeline place and set up branch also at secondary condenser 8 material outlet ends, this also connects vacuum system, and vacuum system is connected with vacuum pump 19.
Described vacuum system is the vacuum buffer tank 16 that is connected with branch by inlet end, be arranged on valve 12 and vacuum breaker 14 in the branch, be arranged on the valve of breathing on the pipeline 11, the underflow valve 18 that is arranged on vacuum buffer tank 16 lower ends constitutes.
Described vacuum buffer tank 16 is connected with vacuum pump 19, and the pipeline between them is provided with vacuum breaker 17.
Described vacuum buffer tank 16 is provided with vacuumometer 15.
Advantage of the present invention and effect are as follows:
The present invention can reclaim the titanium tetrachloride that remains in the copper wire tower, thereby the loss that has reduced titanium tetrachloride has improved the casting yield of material.Prolong the life-span of copper wire tower, reduced the spent acid water yield.
Because the titanium tetrachloride of emitting with copper wire balls reduces, the hydrochloric acid that makes the titanium tetrachloride hydrolysis reaction produce reduces.Having improved the Working environment in the workshop has also reduced because of the corrosion of hydrochloric acid gas to facilities such as the building in the workshop, equipment and pipelines simultaneously.
Description of drawings
Fig. 1 is the process flow sheet that the present invention reclaims residual titanium tetrachloride in copper-wire tower.
Fig. 2 is that existing copper wire tower removes the vanadium process flow sheet.
Among the figure: 1. valve, 2. flow control valve, 3. still kettle, 4. underflow valve, 5. surplus valve, 6. copper wire tower, 7. first-stage condenser, 8. secondary condenser, 9. phlegma buffering storage tank, 10. valve, 11. valve, 12. valves, 13. vacuumometers, 14. vacuum breaker, 15. vacuumometers, 16. vacuum buffer tanks, 17. vacuum breaker, 18. underflow valves, 19. vacuum pumps.
Embodiment
As shown in Figure 1, the present invention reclaims the method for residual titanium tetrachloride in copper-wire tower, respiratory siphon pass after original copper wire tower is except that secondary condenser in the vanadium technology goes out branch, and connection vacuum system, before the copper wire balls manipulation of regeneration, titanium tetrachloride residual in the copper wire tower is reclaimed, the negative pressure of utilizing vacuum system to produce makes the titanium tetrachloride that remains in the copper wire tower lean on the vapour pressure of self to be evaporated to condenser, because the low temperature of condenser and secondary condenser makes titanium tetrachloride be condensed and is collected into phlegma buffering storage tank.
It is as follows that the present invention reclaims the concrete grammar of residual titanium tetrachloride in copper-wire tower: when removing after vanadium work carries out for some time, the copper wire surface passivation loses chemically reactive, at this moment needs copper wire balls taken out carry out manipulation of regeneration.Before the copper wire balls manipulation of regeneration, close heating power supply and the valve 1 and the flow control valve 2 of still kettle 3 earlier, open underflow valve 4 the more a part of titanium tetrachloride in titanium tetrachloride in the still kettle 4 and the copper wire tower 6 is expelled to except that titanium tetrachloride storage tank before the vanadium, close underflow valve 4 then; Shut-off valve 10 and valve 11 are also opened valve 12, start vacuum pump 19, the vacuum tightness of measuring according to the vacuumometer on the vacuum buffer tank 16 15 and control vacuum breaker 17 automatically, after reaching requirement, vacuum tightness closes sky variable valve 17 automatically, titanium tetrachloride vapors is pressed with the pass under vacuum requirements and the differing temps, when temperature was in 10～50 ℃, vacuum tightness should be at 700～5000Pa; When temperature was in 50～136 ℃, vacuum tightness should be at 5000～50000Pa; Valve 12 places behind secondary condenser are provided with vacuumometer 13, automatically control vacuum breaker 14 according to the vacuum tightness of measuring, make that vacuum tightness is neither too high low only herein, titanium tetrachloride vapors is pressed with the pass under this vacuum tightness and the differing temps, when temperature was in 10～50 ℃, vacuum tightness should be at 700～5000Pa; When temperature was in 50～136 ℃, vacuum tightness should be at 5000～50000Pa; Thereby, the too high situation of vacuum tightness make the argon gas of breathing in the piping system enter reduction vacuum tightness if can opening valve 11; Titanium tetrachloride in the copper wire tower becomes steam by self vapour pressure effect under vacuum and normal temperature (or being higher than normal temperature) state, vapour temperature descends because of the heat-eliminating medium effect after steam enters condenser 7 and 8, because temperature reduction titanium tetrachloride vapors is pressed also reduction to make gaseous titanium tetrachloride be condensed into liquid state and is collected into phlegma buffering storage tank 9; After recovery operation is finished, close vacuum breaker 17, close vacuum pump 19; Open valve 11, open underflow valve 18 then, emit and may enter in the vacuum buffer tank 16 and the titanium tetrachloride that condenses and, shut-off valve 18 again; Close vacuum breaker 14 and valve 12.
The system architecture that the present invention reclaims residual titanium tetrachloride in copper-wire tower is as follows: it comprises still kettle 3, copper wire tower 6, first-stage condenser 7, secondary condenser 8 and phlegma buffering storage tank 9, wherein connect breathing pipeline place and set up branch also at secondary condenser 8 material outlet ends, this also connects vacuum system, and vacuum system is connected with vacuum pump 19.
Described vacuum system is the vacuum buffer tank 16 that is connected with branch by inlet end, be arranged on valve 12 and vacuum breaker 14 in the branch, be arranged on the valve of breathing on the pipeline 11, the underflow valve 18 that is arranged on vacuum buffer tank 16 lower ends constitutes.Vacuum buffer tank 16 is connected with vacuum pump 19, and the pipeline between them is provided with vacuum breaker 17.Vacuum buffer tank 16 is provided with vacuumometer 15.
Claims (9)
1, a kind of method that reclaims residual titanium tetrachloride in copper-wire tower, it is characterized in that the respiratory siphon pass after original copper wire tower is except that secondary condenser in the vanadium technology goes out branch, and connection vacuum system, before the copper wire balls manipulation of regeneration, titanium tetrachloride residual in the copper wire tower is reclaimed, the negative pressure of utilizing vacuum system to produce makes the titanium tetrachloride that remains in the copper wire tower lean on the vapour pressure of self to be evaporated to condenser, because the low temperature of condenser and secondary condenser makes titanium tetrachloride be condensed and is collected into phlegma buffering storage tank.
2, the method for recovery residual titanium tetrachloride in copper-wire tower according to claim 1, it is characterized in that it is heating power supply and the valve (1) and the flow control valve (2) of closing still kettle (3) earlier, open underflow valve (4) again titanium tetrachloride in the still kettle (4) and a part of titanium tetrachloride in the copper wire tower (6) are expelled to except that titanium tetrachloride storage tank before the vanadium, close underflow valve (4) then; Shut-off valve (10) and valve (11) are also opened valve (12), start vacuum pump (19), the vacuum tightness in the control vacuum buffer tank (16); Titanium tetrachloride in the copper wire tower (6) is at vacuum and normal temperature or be higher than under the state of normal temperature by self vapour pressure effect and become steam, vapour temperature descends because of the heat-eliminating medium effect after steam enters first-stage condenser (7) and secondary condenser (8), because temperature reduction titanium tetrachloride vapors is pressed also reduction to make gaseous titanium tetrachloride be condensed into liquid state and is collected into phlegma buffering storage tank (9), recovery operation is finished.
3, the method for the described recovery residual titanium tetrachloride in copper-wire tower of claim 2, it is characterized in that vacuum tightness in the described control vacuum buffer tank (16) is the vacuum tightness of measuring according to the vacuumometer (15) on the vacuum buffer tank (16) and control vacuum breaker (17) automatically, closes sky variable valve (17) automatically after vacuum tightness reaches requirement; Valve behind secondary condenser (12) locates to be provided with vacuumometer (13), controls vacuum breaker (14) automatically according to the vacuum tightness of measuring, and makes that vacuum tightness is neither too high low only herein.
4, the method for the described recovery residual titanium tetrachloride in copper-wire tower of claim 3, it is characterized in that the vacuum tightness of described measurement too high then open valve (11) thus make that breathing argon gas in the piping system enters and reduce vacuum tightness.
5, the method for the described recovery residual titanium tetrachloride in copper-wire tower of claim 2 is characterized in that after described recovery operation is finished, and closes vacuum breaker (17), closes vacuum pump (19); Open valve (11), open underflow valve (18) then, emit and to enter in the vacuum buffer tank (16) and the titanium tetrachloride that condenses and, shut-off valve (18) again; Close vacuum breaker (14) and valve (12).
6, a kind of system that reclaims residual titanium tetrachloride in copper-wire tower, it comprises still kettle (3), copper wire tower (6), first-stage condenser (7), secondary condenser (8) and phlegma buffering storage tank (9), it is characterized in that connecting breathing pipeline place at secondary condenser (8) material outlet end sets up branch also, this also connects vacuum system, and vacuum system is connected with vacuum pump (19).
7, the system of the described recovery residual titanium tetrachloride in copper-wire tower of claim 6, it is characterized in that described vacuum system be the vacuum buffer tank (16) that is connected with branch by inlet end, be arranged on valve (12) and vacuum breaker (14) in the branch, be arranged on the valve of breathing on the pipeline (11), the underflow valve (18) that is arranged on vacuum buffer tank (16) lower end constitutes.
8, the system of the described recovery residual titanium tetrachloride in copper-wire tower of claim 7 is characterized in that being connected with vacuum pump (19) of described vacuum buffer tank (16), and the pipeline between them is provided with vacuum breaker (17).
9, the system of claim 7 or 8 described recovery residual titanium tetrachloride in copper-wire tower is characterized in that described vacuum buffer tank (16) is provided with vacuumometer (15).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100125800A CN101638248B (en) | 2008-08-01 | 2008-08-01 | Method and system for recovering residual titanium tetrachloride in copper-wire tower |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100125800A CN101638248B (en) | 2008-08-01 | 2008-08-01 | Method and system for recovering residual titanium tetrachloride in copper-wire tower |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101638248A true CN101638248A (en) | 2010-02-03 |
| CN101638248B CN101638248B (en) | 2012-03-28 |
Family
ID=41613457
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100125800A Expired - Fee Related CN101638248B (en) | 2008-08-01 | 2008-08-01 | Method and system for recovering residual titanium tetrachloride in copper-wire tower |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101638248B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106946286A (en) * | 2017-03-09 | 2017-07-14 | 金川集团股份有限公司 | A kind of crude titanic chloride is except the chemical reaction equipment and method of vanadium |
| CN107267765A (en) * | 2017-08-17 | 2017-10-20 | 东方弗瑞德（北京）科技有限公司 | A kind of method that copper is reclaimed from copper wire waste liquid is washed |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100376699C (en) * | 2006-07-28 | 2008-03-26 | 遵义钛业股份有限公司 | Copper wire tower having supporting device used for removing vanadium impurity in titanium tetrachloride |
| CN101205801A (en) * | 2007-11-22 | 2008-06-25 | 陈敏 | Pumping unit polish rod centralized connecting device |
-
2008
- 2008-08-01 CN CN2008100125800A patent/CN101638248B/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106946286A (en) * | 2017-03-09 | 2017-07-14 | 金川集团股份有限公司 | A kind of crude titanic chloride is except the chemical reaction equipment and method of vanadium |
| CN107267765A (en) * | 2017-08-17 | 2017-10-20 | 东方弗瑞德（北京）科技有限公司 | A kind of method that copper is reclaimed from copper wire waste liquid is washed |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101638248B (en) | 2012-03-28 |
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Granted publication date: 20120328 |